Recycling of [(18)O]water for [(18)F]fluoride production can be accomplished with reliable results. We have developed sensitive, robust, and rapid analyses of impurities in [(18)O]water. Anions were quantitated by capillary electrophoresis and organic residuals were quantitated by gas chromatography using methods with excellent reproducibility and linearity. Kryptofix 222 (K-222) was quantitated by a sensitive LC-MS-MS technique. Isotopic composition was determined by GC-MS with satisfactory accuracy and precision. These methods were employed to evaluate recovered [(18)O]water purified by a novel electrolysis method. 2-[(18)F]FDG yields using purified [(18)O]water with very low levels of impurities are indistinguishable from newly purchased [(18)O]water. High (> 300 ppm) carbonate concentration reduces the fluoride trapping efficiency of QMA. The analyses of anions, organics, and isotopic enrichment were applied routinely for quality control of [(18)O]water to predict a satisfactory outcome of 2-[(18)F]FDG production.